反応 #213920

ord-ed3f9eaae94f4193abd114e291ec9a02

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONA mixture of 10.0 g
  2. 2
    workup.DISTILLATIONThe excess hydride is distilled off
  3. 3
    workup.DISTILLATIONthe residue is purified by molecular distillation (bath temperature=170°-175° C., 0.2mm.)
  4. 4
    その他to give 20.5 g

実験手順

A mixture of 10.0 g. (36.7 mmoles) of 4-dimethoxymethyl-4-trimethylsiloxy-1-octyne, 12.82 g. (44 mmoles) of tri-n-butylstannyl hydride 100 mg. of azobisisobutyronitrile is heated to 140° C. under argon for 2 hours. The excess hydride is distilled off and the residue is purified by molecular distillation (bath temperature=170°-175° C., 0.2mm.) to give 20.5 g. of the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04254036uspto-grants-1981_03